CN106629860B - A kind of preparation method of the 2D type Multiferroic composite materials of cobalt ferrite/lead titanates 0 - Google Patents

A kind of preparation method of the 2D type Multiferroic composite materials of cobalt ferrite/lead titanates 0 Download PDF

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CN106629860B
CN106629860B CN201611107685.5A CN201611107685A CN106629860B CN 106629860 B CN106629860 B CN 106629860B CN 201611107685 A CN201611107685 A CN 201611107685A CN 106629860 B CN106629860 B CN 106629860B
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CN106629860A (en
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任召辉
沈烨婷
李玮
武梦姣
沈鸽
韩高荣
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Zhejiang University ZJU
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    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
    • C04B35/2666—Other ferrites containing nickel, copper or cobalt
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    • C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
    • C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
    • C04B35/472—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on lead titanates
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Abstract

The invention discloses a kind of preparation method of the 2D type Multiferroic composite materials of cobalt ferrite/lead titanates 0.This method is to be used as primary raw material using cabaltous nitrate hexahydrate, Fe(NO3)39H2O and lead titanates nanometer sheet, monohydrate potassium is as complexing agent, dispersant, by the use of ammoniacal liquor as pH adjusting agent, CoFe is realized by allocating the amount of every raw material, and using the method for collosol and gel solid-phase sintering2O4/PbTiO3The synthesis of Multiferroic composite material.The multi-iron material that such a preparation method obtains is without clamping effect, and the complex method of ferromagnetic phase and ferroelectric phase is 0 novel 2D types, i.e. the CoFe of zero dimension2O4Particle and the PbTiO of two dimension3Nanometer sheet is compound, and its magnetoelectric effect has potential application in various fields.

Description

A kind of preparation method of cobalt ferrite/lead titanates 0-2D type Multiferroic composite materials
Technical field
The invention belongs to functional material preparation field, is related to a kind of CoFe2O4/PbTiO30-2D type Multiferroic composite materials Preparation method.
Background technology
With the rapid development of information technology, requiring that memory technology provides speed faster, capacity is bigger, and power consumption is lower, body Product is smaller, and the life-span is longer, the higher memory of reliability, and preparation of the magnetoelectric effect also for memory of future generation provides theory Support.
Compound multi-ferroic material has many obvious advantages, compound by regulating and controlling ratio, the control synthesis condition of component Multi-ferroic material can effectively control ferroelectricity, magneto-electric property and magnetoelectric effect, therefore have extensive prospect.But base The clamping effect of plate is larger, stress transmission is difficult, interface damage is serious and the factors such as preparation technology is relative complex make magneto-electric coupled effect The optimization answered is limited by very large, and also governs the practical application of the compound multi-iron material of ferroelectric-ferromagnetic.
Different from generally preparing the physical deposition method such as PLD used by magnetoelectric composite film, the present invention is using colloidal sol-solidifying Glue solid sintering technology prepares more iron composite materials.In this preparation method, due to no introducing substrate, substrate would not be brought To the clamping action of ferroelectric phase (ferromagnetic phase).It is expected that by eliminating clamping action, considerable magnetoelectric effect can be obtained.
PbTiO3Single crystal nanoplate provides to prepare the two-dimentional ferroelectric-ferromagnetic composite with homogeneous single crystal hetero-junctions May.In addition, CoFe2O4Because it has high-magnetostriction performance, magnetic anisotropy, suitable saturated magnetization strong at room temperature Degree, high-coercive force, high resistivity and fabulous heat endurance, are also widely used as ferromagnetism group in magneto-electric coupled composite Point.
The content of the invention
CoFe is realized using the method for collosol and gel-solid-phase sintering2O4/PbTiO3The synthesis of Multiferroic composite material, it is such a For the multi-iron material that preparation method obtains without clamping effect, the complex method of ferromagnetic phase and ferroelectric phase is new 0-2D types.This hair Bright to provide a kind of preparation method of cobalt ferrite/lead titanates 0-2D type Multiferroic composite materials, preparation method comprises the following steps：
1) in molar ratio 1:2:9, which weigh cabaltous nitrate hexahydrate, Fe(NO3)39H2O, monohydrate potassium, is dissolved in deionization In water, stir and evenly mix；
2) ammoniacal liquor is added dropwise dropwise into step 1) resulting solution, until solution ph is changed into 7；
3) by PbTiO3Nanometer sheet adds step 2) resulting solution, mixes 5min；
4) step 3) resulting solution is heated to 90 DEG C and continues 30~45min of stirring, solution start retrogradation to colloidal sol after And it is changed into gel；
5) gel obtained by step 4) is transferred to crucible, is put into Muffle furnace and is heated to 240 DEG C of insulation 4h；
6) it will be clayed into power after block loose product cooling obtained by step 5) with mortar, be placed again into Muffle furnace and be heated to 570 DEG C of insulation 4h, final product is obtained after cooling.
Raw material cabaltous nitrate hexahydrate, Fe(NO3)39H2O monohydrate potassium, ammoniacal liquor and deionized water used in the present invention Purity not less than chemistry it is pure.Lead titanates is the nanometer sheet of monocrystalline one-domain structure, has well-regulated rectangle pattern, lateral dimension For 600~1100nm, thickness is 120~180nm.
Further, the stirring of step 1~5 is carried out at room temperature.
Further, CoFe in products therefrom2O4Component is particle of the size in 10~200nm.
The PbTiO of heretofore described monocrystalline one-domain structure3The preparation method of nanometer sheet refers to patent The preparation method of ZL201210036177.8 --- perovskite lead titanate single-crystal nanometer sheet.
The beneficial effects of the invention are as follows：
The CoFe prepared using the inventive method2O4/PbTiO3Composite is new 0-2D type multiferroic materials Material, the i.e. CoFe of zero dimension2O4Particle and the PbTiO of two dimension3Nanometer sheet is compound, and the multi-iron material is without clamping effect.
Brief description of the drawings
CoFe prepared by Fig. 1 (a) examples 1, (b) example 32O4/PbTiO3The X-ray diffraction of Multiferroic composite material (XRD) collection of illustrative plates；
CoFe prepared by Fig. 2 (a) examples 1, (b) example 32O4/PbTiO3The scanning electron microscopy of Multiferroic composite material Mirror (SEM) photo；
CoFe prepared by Fig. 3 examples 12O4/PbTiO3The transmission electron microscope of Multiferroic composite material heterojunction boundary (TEM) photo；
CoFe prepared by Fig. 4 examples 12O4/PbTiO3The M-H hysteresis curves of Multiferroic composite material.
Embodiment
The present invention is further illustrated below in conjunction with example.
Embodiment 1
Synthesize CoFe2O4/PbTiO3Mol ratio is 1/8 composite.
Carry out in following processing steps.
1) weigh cabaltous nitrate hexahydrate, Fe(NO3)39H2O, monohydrate potassium respectively to be dissolved in deionized water, it rubs Your concentration is respectively 0.0313mol/L, 0.0626mol/L, 0.2819mol/L, stirs 10min, wherein molar concentration volume Radix is slurry cumulative volume；
2) ammoniacal liquor is added dropwise dropwise into step 1) resulting solution, until solution ph is changed into 7；
3) by PbTiO3Nanometer sheet adds step 2) resulting solution, wherein, PbTiO3Addition be cabaltous nitrate hexahydrate thing 8 times of the amount of matter, mix 5min；
4) step 3) resulting solution is heated to 90 DEG C and continues to stir 30min, solution starts retrogradation and then become to colloidal sol For gel；
5) gel obtained by step 4) is transferred to crucible, is put into Muffle furnace and is heated to 240 DEG C of insulation 4h；
6) it will be clayed into power after block loose product cooling obtained by step 5) with mortar, be placed again into Muffle furnace and be heated to 570 DEG C of insulation 4h, final product is obtained after cooling.X-ray diffraction (XRD) collection of illustrative plates of synthesized composite is shown in Fig. 1 (a)； Its SEM (SEM) photo is shown in Fig. 2 (a)；Transmission electron microscope (TEM) photo of its compound interface is shown in figure 3；Its M-H hysteresis curve is shown in Fig. 4.It can be seen that：CoFe2O4Granular size is in 10~20nm, and its homoepitaxial is in PbTiO3's (001) on plane of polarization.Its cross sectional shape is triangle, has certain facet, can be seen that in addition from M-H hysteresis curves CoFe2O4/PbTiO3Composite still has ferromagnetism.
Embodiment 2
Synthesize CoFe2O4/PbTiO3Mol ratio is 1/4 composite.
Specific processing step is identical with example 1, and difference is：Cabaltous nitrate hexahydrate, nine water nine hydration nitre in step 1) Sour iron, the molar concentration of monohydrate potassium are respectively 0.0626mol/L, 0.1252mol/L, 0.5638mol/L,；Step 3) Middle PbTiO3Addition be 4 times of amount of cabaltous nitrate hexahydrate material.
Embodiment 3
Synthesize CoFe2O4/PbTiO3Mol ratio is 2/4 composite.
Specific processing step is identical with example 1, and difference is：Cabaltous nitrate hexahydrate, nine water nine hydration nitre in step 1) Sour iron, the molar concentration of monohydrate potassium are respectively 0.1252mol/L, 0.2504mol/L, 1.1276mol/L,；Step 3) Middle PbTiO3Addition be 2 times of amount of cabaltous nitrate hexahydrate material；Stirring 45min in step 4).Synthesized composite X-ray diffraction (XRD) collection of illustrative plates be shown in Fig. 1 (b)；Its SEM (SEM) photo is shown in Fig. 2 (b).
Embodiment 4
Synthesize CoFe2O4/PbTiO3Mol ratio is 3/4 composite.
Specific processing step is identical with example 1, and difference is：Cabaltous nitrate hexahydrate, nine water nine hydration nitre in step 1) Sour iron, the molar concentration of monohydrate potassium are respectively 0.1878mol/L, 0.3756mol/L, 1.6914mol/L,；Step 3) Middle PbTiO3Addition be 4/3 times of amount of cabaltous nitrate hexahydrate material；Stirring 45min in step 4).

Claims (5)

1.CoFe2O4/PbTiO3The preparation method of 0-2D type Multiferroic composite materials, it is characterized in that, comprise the following steps：
1) in molar ratio 1:2:9, which weigh cabaltous nitrate hexahydrate, Fe(NO3)39H2O, monohydrate potassium, is dissolved in deionized water In, stir and evenly mix；
2) ammoniacal liquor is added dropwise dropwise into step 1) resulting solution, until solution ph is changed into 7；
3) by PbTiO3Nanometer sheet adds step 2) resulting solution, mixes 5min；
4) step 3) resulting solution is heated to 90 DEG C and continues 30~45min of stirring, solution starts retrogradation and then become to colloidal sol For gel；
5) gel obtained by step 4) is transferred to crucible, is put into Muffle furnace and is heated to 240 DEG C of insulation 4h；
6) it will be clayed into power after block loose product cooling obtained by step 5) with mortar, be placed again into Muffle furnace and be heated to 570 DEG C 4h is incubated, final product is obtained after cooling.
2. CoFe according to claim 12O4/PbTiO3The preparation method of 0-2D type Multiferroic composite materials, its feature It is that raw material cabaltous nitrate hexahydrate used, Fe(NO3)39H2O monohydrate potassium, the purity of ammoniacal liquor and deionized water is not low It is pure in chemistry.
3. CoFe according to claim 12O4/PbTiO3The preparation method of 0-2D type Multiferroic composite materials, its feature It is that the stirring of step 1~5 is carried out at room temperature.
4. CoFe according to claim 12O4/PbTiO3The preparation method of 0-2D type Multiferroic composite materials, its feature It is CoFe in final product2O4Component is particle of the size in 10~200nm.
5. CoFe according to claim 12O4/PbTiO3The preparation method of 0-2D type Multiferroic composite materials, its feature It is that described lead titanates nanometer sheet is the nanometer sheet of monocrystalline one-domain structure, has well-regulated rectangle pattern, lateral dimension 600 ~1100nm, thickness are 120~180nm.
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CN108588834B (en) * 2018-05-25 2020-11-13 许昌学院 Two-dimensional single crystal PbTiO with strong magnetic electric coupling effect3-CoFe2O4Preparation method of composite nano material

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102173763A (en) * 2011-01-11 2011-09-07 桂林理工大学 Bismuth ferrititanate multiferroic material and sol-gel preparation method thereof
CN102173764A (en) * 2011-01-11 2011-09-07 桂林理工大学 Bismuth-ferrite-base multiferroic material and preparation method thereof
CN102531595A (en) * 2011-12-23 2012-07-04 常州大学 Preparation method for 0-3 compound multiple-ferrite ceramic of cobalt ferrite and lead lanthanum zironate titanate
CN103130281A (en) * 2013-03-15 2013-06-05 北京航空航天大学 Chemical preparation method of multiferroic BiFeO3 doped film
CN104128184A (en) * 2014-06-24 2014-11-05 安徽理工大学 Floating type CoFe2O4/TiO2/floating bead composite photocatalyst and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102173763A (en) * 2011-01-11 2011-09-07 桂林理工大学 Bismuth ferrititanate multiferroic material and sol-gel preparation method thereof
CN102173764A (en) * 2011-01-11 2011-09-07 桂林理工大学 Bismuth-ferrite-base multiferroic material and preparation method thereof
CN102531595A (en) * 2011-12-23 2012-07-04 常州大学 Preparation method for 0-3 compound multiple-ferrite ceramic of cobalt ferrite and lead lanthanum zironate titanate
CN103130281A (en) * 2013-03-15 2013-06-05 北京航空航天大学 Chemical preparation method of multiferroic BiFeO3 doped film
CN104128184A (en) * 2014-06-24 2014-11-05 安徽理工大学 Floating type CoFe2O4/TiO2/floating bead composite photocatalyst and preparation method thereof

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